Methanol → 2-(Methoxymethyl)-4-nitrophenol

HRID 268550

反応式

HRID 268550 の反応式
Cl[CH2:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=1[OH:12].[CH3:13][OH:14].C[O-].[Na+]>O>[CH3:13][O:14][CH2:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=1[OH:12]

参加物

5

反応物 3

HCID 887MethanolHCID 763052-(Chloromethyl)-4-nitrophenolHCID 10942334Sodium Methoxide

生成物 1

HCID 113558782-(Methoxymethyl)-4-nitrophenol

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

18.7 g (0.1 mol) of 2-chloromethyl-4-nitrophenol and 50 ml of pure methanol were mixed together and refluxed for 2 hours 30 minutes. 37 ml of sodium methoxide (0.2 mol, 5.4 N solution in MeOH) were added and the mixture was refluxed for another 30 minutes. The resulting mixture was cooled in an ice bath and diluted with 350 ml of water, and the insoluble matter formed was filtered off. The filtrate was acidified with acetic acid (10 ml). The crystalline product was filtered off by suction, reslurried in ice-cold water and then dried over P2O5 at 40° C. 11.4 g of crude products were isolated and then recrystallized from 15 ml of isopropyl acetate to give 7.5 g of expected product.

後処理

  1. temperaturerefluxed for 2 hours 30 minutes
  2. temperaturethe mixture was refluxed for another 30 minutes
  3. temperatureThe resulting mixture was cooled in an ice bath
  4. customthe insoluble matter formed
  5. filtrationwas filtered off
  6. filtrationThe crystalline product was filtered off by suction
  7. dry with materialdried over P2O5 at 40° C
  8. custom11.4 g of crude products were isolated
  9. customrecrystallized from 15 ml of isopropyl acetate

出典と根拠

ORDレコード
ord-0a0551b5bf3049c0a58006b54583054c
出典データセット
uspto-grants-2008_11
特許番号
US07445645B2

関連ノート

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